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The title compound, (NH
4)
2[Na
2Ni(OH)
6Mo
6O
18(H
2O)
2], features inversion-generated hexamolybdonickelate(II) anions (Ni site symmetry
). The anions are linked by the five-coordinate sodium cations into layers. Adjacent layers are linked through N—H
O and O—H
O hydrogen bonds involving the ammonium ions and water molecules, thus forming a three-dimensional network.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (a-O) = 0.015 Å
- R factor = 0.056
- wR factor = 0.098
- Data-to-parameter ratio = 14.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT416_ALERT_2_B Short Intra D-H..H-D H2 .. H2 .. 1.10 Ang.
PLAT420_ALERT_2_B D-H Without Acceptor O1 - H1 ... ?
PLAT420_ALERT_2_B D-H Without Acceptor O3 - H3 ... ?
PLAT420_ALERT_2_B D-H Without Acceptor OW3 - HW3B ... ?
Alert level C
PLAT213_ALERT_2_C Atom O6 has ADP max/min Ratio ............. 3.80 oblat
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.52 Ratio
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 84.00 A 3
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 13
0 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
7 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.
Poly[diammonium hexahydroxyoctadecaoxodisodiohexamolybdonickelate dihydrate]
top
Crystal data top
(NH4)2[Na2Ni(OH)6Mo6O18]·2H2O | F(000) = 1164 |
Mr = 1214.54 | Dx = 2.964 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yc | Cell parameters from 7685 reflections |
a = 11.7792 (10) Å | θ = 0.3–0.7° |
b = 10.9353 (9) Å | µ = 3.50 mm−1 |
c = 11.7793 (10) Å | T = 296 K |
β = 116.223 (4)° | Block, light green |
V = 1361.1 (2) Å3 | 0.16 × 0.12 × 0.11 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD APEX II diffractometer | 2674 independent reflections |
Radiation source: fine-focus sealed tube | 1396 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
ω scans | θmax = 26.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −13→14 |
Tmin = 0.605, Tmax = 0.680 | k = −13→13 |
7181 measured reflections | l = −12→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.038P)2] where P = (Fo2 + 2Fc2)/3 |
2674 reflections | (Δ/σ)max < 0.001 |
187 parameters | Δρmax = 0.75 e Å−3 |
0 restraints | Δρmin = −0.67 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni | 0.5000 | 0.0000 | 0.0000 | 0.0203 (5) | |
Mo1 | 0.66140 (9) | 0.23128 (9) | 0.17284 (9) | 0.0236 (3) | |
Mo2 | 0.18736 (9) | 0.00712 (9) | −0.13713 (10) | 0.0254 (3) | |
Mo3 | 0.34982 (9) | 0.23942 (9) | 0.03826 (9) | 0.0234 (3) | |
Na | 0.9161 (9) | 0.3036 (9) | 0.0681 (10) | 0.041 (2) | |
O1 | 0.6445 (7) | 0.1090 (6) | 0.0168 (7) | 0.0209 (18) | |
H1 | 0.6418 | 0.1459 | −0.0501 | 0.025* | |
O2 | 0.5023 (7) | 0.1086 (6) | 0.1401 (7) | 0.0216 (18) | |
H2 | 0.5026 | 0.0683 | 0.2045 | 0.026* | |
O3 | 0.3572 (7) | 0.1142 (6) | −0.1057 (7) | 0.0225 (19) | |
H3 | 0.3600 | 0.1514 | −0.1701 | 0.027* | |
O4 | 0.7677 (7) | 0.0902 (7) | 0.2457 (7) | 0.028 (2) | |
O5 | 0.7639 (7) | 0.3216 (6) | 0.1453 (8) | 0.033 (2) | |
O6 | 0.6677 (7) | 0.2872 (7) | 0.3064 (7) | 0.032 (2) | |
O7 | 0.5069 (7) | 0.3068 (6) | 0.0507 (7) | 0.0244 (19) | |
O8 | 0.3515 (7) | 0.2902 (7) | 0.1731 (7) | 0.032 (2) | |
O9 | 0.2531 (7) | 0.3397 (7) | −0.0730 (8) | 0.033 (2) | |
O10 | 0.2343 (7) | 0.1050 (6) | 0.0124 (7) | 0.0259 (19) | |
O11 | 0.0886 (7) | 0.1044 (7) | −0.2473 (8) | 0.036 (2) | |
O12 | 0.0900 (7) | −0.0897 (7) | −0.1066 (8) | 0.039 (2) | |
OW1 | 0.9912 (11) | 0.2577 (10) | −0.0731 (11) | 0.048 (2) | |
HW1A | 0.9470 | 0.2645 | −0.1555 | 0.057* | |
HW1B | 1.0551 | 0.2294 | −0.0796 | 0.057* | |
OW2 | 0.4796 (9) | 0.0467 (7) | 0.3465 (8) | 0.053 (3) | |
HW2A | 0.4068 | 0.0235 | 0.3251 | 0.064* | |
HW2B | 0.5186 | −0.0010 | 0.4165 | 0.064* | |
OW3 | 0.8692 (9) | 0.4746 (10) | −0.0089 (9) | 0.082 (4) | |
HW3A | 0.8921 | 0.5422 | 0.0318 | 0.099* | |
HW3B | 0.8691 | 0.4982 | −0.0770 | 0.099* | |
N | 0.1695 (9) | 0.0346 (8) | 0.1939 (9) | 0.040 (3) | |
HN1 | 0.2009 | 0.0386 | 0.1421 | 0.048* | |
HN2 | 0.2021 | 0.1014 | 0.2474 | 0.048* | |
HN3 | 0.2019 | −0.0199 | 0.2500 | 0.048* | |
HN4 | 0.0901 | 0.0386 | 0.1589 | 0.048* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni | 0.0232 (12) | 0.0228 (11) | 0.0154 (11) | −0.0013 (10) | 0.0090 (9) | −0.0017 (10) |
Mo1 | 0.0287 (6) | 0.0229 (6) | 0.0181 (6) | −0.0044 (5) | 0.0094 (5) | −0.0062 (5) |
Mo2 | 0.0227 (6) | 0.0285 (6) | 0.0215 (6) | 0.0015 (6) | 0.0066 (5) | −0.0025 (5) |
Mo3 | 0.0294 (6) | 0.0221 (6) | 0.0189 (6) | 0.0040 (5) | 0.0108 (5) | −0.0011 (5) |
Na | 0.041 (2) | 0.040 (2) | 0.042 (2) | −0.0002 (10) | 0.0175 (14) | 0.0002 (10) |
O1 | 0.029 (5) | 0.018 (4) | 0.014 (4) | 0.002 (3) | 0.007 (4) | 0.004 (3) |
O2 | 0.028 (5) | 0.024 (4) | 0.011 (4) | 0.000 (4) | 0.007 (4) | 0.001 (3) |
O3 | 0.024 (5) | 0.021 (4) | 0.014 (4) | 0.002 (4) | 0.000 (4) | −0.002 (3) |
O4 | 0.031 (5) | 0.036 (5) | 0.014 (4) | 0.000 (4) | 0.008 (4) | −0.001 (4) |
O5 | 0.032 (5) | 0.029 (5) | 0.041 (6) | −0.002 (4) | 0.018 (5) | −0.004 (4) |
O6 | 0.040 (5) | 0.032 (5) | 0.019 (5) | −0.001 (4) | 0.009 (4) | −0.020 (4) |
O7 | 0.026 (5) | 0.025 (4) | 0.023 (5) | 0.004 (4) | 0.012 (4) | 0.003 (4) |
O8 | 0.042 (6) | 0.035 (5) | 0.021 (5) | 0.006 (4) | 0.015 (4) | −0.009 (4) |
O9 | 0.035 (6) | 0.037 (5) | 0.030 (5) | 0.007 (4) | 0.016 (4) | 0.005 (4) |
O10 | 0.027 (5) | 0.032 (5) | 0.020 (5) | 0.002 (4) | 0.011 (4) | −0.004 (4) |
O11 | 0.033 (6) | 0.043 (5) | 0.024 (5) | 0.017 (4) | 0.005 (4) | 0.000 (4) |
O12 | 0.028 (6) | 0.047 (5) | 0.040 (6) | −0.003 (4) | 0.013 (5) | −0.009 (5) |
OW1 | 0.048 (3) | 0.049 (3) | 0.048 (3) | 0.0015 (10) | 0.0226 (15) | −0.0011 (10) |
OW2 | 0.100 (9) | 0.037 (5) | 0.030 (6) | 0.002 (5) | 0.035 (6) | 0.008 (4) |
OW3 | 0.077 (9) | 0.118 (10) | 0.042 (7) | −0.013 (7) | 0.019 (6) | −0.023 (7) |
N | 0.037 (7) | 0.058 (7) | 0.028 (6) | 0.003 (6) | 0.019 (5) | 0.003 (6) |
Geometric parameters (Å, º) top
Ni—O1 | 2.015 (7) | Mo3—O7 | 1.935 (7) |
Ni—O3 | 2.022 (7) | Mo3—O2 | 2.193 (7) |
Ni—O2 | 2.023 (7) | Mo3—O3 | 2.211 (7) |
Ni—O1i | 2.015 (7) | Na—OW3 | 2.045 (14) |
Ni—O3i | 2.022 (7) | Na—OW1 | 2.258 (16) |
Ni—O2i | 2.023 (7) | Na—O5 | 2.350 (13) |
Mo1—O6 | 1.659 (7) | Na—O12i | 2.389 (13) |
Mo1—O5 | 1.698 (8) | Na—O11ii | 2.442 (13) |
Mo1—O4 | 1.933 (7) | O1—H1 | 0.8740 |
Mo1—O7 | 1.937 (7) | O2—H2 | 0.8764 |
Mo1—O2 | 2.196 (7) | O3—H3 | 0.8742 |
Mo1—O1 | 2.209 (7) | OW1—HW1A | 0.8794 |
Mo2—O11 | 1.684 (8) | OW1—HW1B | 0.8487 |
Mo2—O12 | 1.712 (8) | OW2—HW2A | 0.8195 |
Mo2—O4i | 1.909 (8) | OW2—HW2B | 0.9100 |
Mo2—O10 | 1.922 (7) | OW3—HW3A | 0.8577 |
Mo2—O3 | 2.204 (7) | OW3—HW3B | 0.8422 |
Mo2—O1i | 2.250 (7) | N—HN1 | 0.8438 |
Mo3—O8 | 1.674 (7) | N—HN2 | 0.9301 |
Mo3—O9 | 1.702 (7) | N—HN3 | 0.8446 |
Mo3—O10 | 1.934 (7) | N—HN4 | 0.8406 |
| | | |
O1—Ni—O1i | 180.0 | O2—Mo3—O3 | 73.4 (3) |
O1—Ni—O3i | 82.4 (3) | OW3—Na—OW1 | 89.6 (6) |
O1i—Ni—O3i | 97.6 (3) | OW3—Na—O5 | 89.6 (5) |
O1—Ni—O3 | 97.6 (3) | OW1—Na—O5 | 156.6 (6) |
O1i—Ni—O3 | 82.4 (3) | OW3—Na—O12i | 162.6 (6) |
O3i—Ni—O3 | 180.0 | OW1—Na—O12i | 88.7 (5) |
O1—Ni—O2i | 97.7 (3) | O5—Na—O12i | 85.2 (4) |
O1i—Ni—O2i | 82.3 (3) | OW3—Na—O11ii | 88.5 (5) |
O3i—Ni—O2i | 81.2 (3) | OW1—Na—O11ii | 107.7 (5) |
O3—Ni—O2i | 98.8 (3) | O5—Na—O11ii | 95.6 (5) |
O1—Ni—O2 | 82.3 (3) | O12i—Na—O11ii | 108.5 (5) |
O1i—Ni—O2 | 97.7 (3) | OW3—Na—HW3A | 15.3 |
O3i—Ni—O2 | 98.8 (3) | OW1—Na—HW3A | 98.6 |
O3—Ni—O2 | 81.2 (3) | O5—Na—HW3A | 86.2 |
O2i—Ni—O2 | 180.0 | O12i—Na—HW3A | 171.3 |
O6—Mo1—O5 | 103.2 (4) | O11ii—Na—HW3A | 74.0 |
O6—Mo1—O4 | 97.2 (3) | OW3—Na—HW3B | 15.0 |
O5—Mo1—O4 | 100.0 (3) | OW1—Na—HW3B | 74.9 |
O6—Mo1—O7 | 100.4 (3) | O5—Na—HW3B | 101.9 |
O5—Mo1—O7 | 97.2 (4) | O12i—Na—HW3B | 154.1 |
O4—Mo1—O7 | 151.9 (3) | O11ii—Na—HW3B | 95.6 |
O6—Mo1—O2 | 94.0 (3) | HW3A—Na—HW3B | 28.1 |
O5—Mo1—O2 | 160.9 (3) | Ni—O1—Mo1 | 101.6 (3) |
O4—Mo1—O2 | 85.7 (3) | Ni—O1—Mo2i | 101.4 (3) |
O7—Mo1—O2 | 71.4 (3) | Mo1—O1—Mo2i | 95.0 (3) |
O6—Mo1—O1 | 164.1 (3) | Ni—O1—H1 | 119.5 |
O5—Mo1—O1 | 90.2 (3) | Mo1—O1—H1 | 115.2 |
O4—Mo1—O1 | 71.9 (3) | Mo2i—O1—H1 | 120.0 |
O7—Mo1—O1 | 86.0 (3) | Ni—O2—Mo3 | 103.0 (3) |
O2—Mo1—O1 | 74.2 (3) | Ni—O2—Mo1 | 101.8 (3) |
O11—Mo2—O12 | 104.7 (4) | Mo3—O2—Mo1 | 97.3 (3) |
O11—Mo2—O4i | 97.9 (4) | Ni—O2—H2 | 113.9 |
O12—Mo2—O4i | 101.9 (4) | Mo3—O2—H2 | 119.4 |
O11—Mo2—O10 | 100.1 (3) | Mo1—O2—H2 | 118.6 |
O12—Mo2—O10 | 95.7 (4) | Ni—O3—Mo2 | 102.8 (3) |
O4i—Mo2—O10 | 150.7 (3) | Ni—O3—Mo3 | 102.4 (3) |
O11—Mo2—O3 | 93.5 (3) | Mo2—O3—Mo3 | 96.7 (3) |
O12—Mo2—O3 | 159.4 (3) | Ni—O3—H3 | 118.8 |
O4i—Mo2—O3 | 84.8 (3) | Mo2—O3—H3 | 118.7 |
O10—Mo2—O3 | 71.2 (3) | Mo3—O3—H3 | 114.0 |
O11—Mo2—O1i | 163.4 (3) | Mo2i—O4—Mo1 | 117.7 (4) |
O12—Mo2—O1i | 90.2 (3) | Mo1—O5—Na | 138.9 (5) |
O4i—Mo2—O1i | 71.3 (3) | Mo3—O7—Mo1 | 116.6 (4) |
O10—Mo2—O1i | 85.4 (3) | Mo2—O10—Mo3 | 117.7 (4) |
O3—Mo2—O1i | 73.3 (2) | Mo2—O11—Naiii | 165.1 (5) |
O8—Mo3—O9 | 103.9 (4) | Mo2—O12—Nai | 136.4 (5) |
O8—Mo3—O10 | 96.6 (3) | Na—OW1—HW1A | 124.1 |
O9—Mo3—O10 | 100.6 (3) | Na—OW1—HW1B | 143.1 |
O8—Mo3—O7 | 101.0 (3) | HW1A—OW1—HW1B | 92.7 |
O9—Mo3—O7 | 96.0 (3) | HW2A—OW2—HW2B | 98.2 |
O10—Mo3—O7 | 152.1 (3) | Na—OW3—HW3A | 125.7 |
O8—Mo3—O2 | 92.0 (3) | Na—OW3—HW3B | 126.1 |
O9—Mo3—O2 | 161.6 (3) | HW3A—OW3—HW3B | 97.8 |
O10—Mo3—O2 | 86.5 (3) | HN1—N—HN2 | 105.5 |
O7—Mo3—O2 | 71.5 (3) | HN1—N—HN3 | 114.3 |
O8—Mo3—O3 | 160.9 (3) | HN2—N—HN3 | 96.6 |
O9—Mo3—O3 | 92.8 (3) | HN1—N—HN4 | 113.0 |
O10—Mo3—O3 | 70.9 (3) | HN2—N—HN4 | 109.2 |
O7—Mo3—O3 | 86.2 (3) | HN3—N—HN4 | 116.2 |
| | | |
O3i—Ni—O1—Mo1 | −98.5 (3) | O11—Mo2—O3—Mo3 | 86.8 (3) |
O3—Ni—O1—Mo1 | 81.5 (3) | O12—Mo2—O3—Mo3 | −65.5 (9) |
O2i—Ni—O1—Mo1 | −178.5 (3) | O4i—Mo2—O3—Mo3 | −175.6 (3) |
O2—Ni—O1—Mo1 | 1.5 (3) | O10—Mo2—O3—Mo3 | −12.7 (3) |
O3i—Ni—O1—Mo2i | −0.9 (3) | O1i—Mo2—O3—Mo3 | −103.5 (3) |
O3—Ni—O1—Mo2i | 179.1 (3) | O8—Mo3—O3—Ni | −41.4 (11) |
O2i—Ni—O1—Mo2i | −80.9 (3) | O9—Mo3—O3—Ni | 167.7 (4) |
O2—Ni—O1—Mo2i | 99.1 (3) | O10—Mo3—O3—Ni | −92.1 (4) |
O6—Mo1—O1—Ni | 41.5 (13) | O7—Mo3—O3—Ni | 71.8 (3) |
O5—Mo1—O1—Ni | −170.3 (3) | O2—Mo3—O3—Ni | 0.0 (3) |
O4—Mo1—O1—Ni | 89.2 (3) | O8—Mo3—O3—Mo2 | 63.4 (10) |
O7—Mo1—O1—Ni | −73.2 (3) | O9—Mo3—O3—Mo2 | −87.6 (3) |
O2—Mo1—O1—Ni | −1.4 (3) | O10—Mo3—O3—Mo2 | 12.7 (3) |
O6—Mo1—O1—Mo2i | −61.3 (12) | O7—Mo3—O3—Mo2 | 176.5 (3) |
O5—Mo1—O1—Mo2i | 86.9 (3) | O2—Mo3—O3—Mo2 | 104.7 (3) |
O4—Mo1—O1—Mo2i | −13.5 (3) | O6—Mo1—O4—Mo2i | −173.7 (4) |
O7—Mo1—O1—Mo2i | −176.0 (3) | O5—Mo1—O4—Mo2i | −68.8 (5) |
O2—Mo1—O1—Mo2i | −104.2 (3) | O7—Mo1—O4—Mo2i | 57.9 (8) |
O1—Ni—O2—Mo3 | 98.9 (3) | O2—Mo1—O4—Mo2i | 92.9 (4) |
O1i—Ni—O2—Mo3 | −81.1 (3) | O1—Mo1—O4—Mo2i | 18.1 (4) |
O3i—Ni—O2—Mo3 | 180.0 (3) | O6—Mo1—O5—Na | 141.9 (7) |
O3—Ni—O2—Mo3 | 0.0 (3) | O4—Mo1—O5—Na | 42.0 (8) |
O1—Ni—O2—Mo1 | −1.5 (3) | O7—Mo1—O5—Na | −115.6 (8) |
O1i—Ni—O2—Mo1 | 178.5 (3) | O2—Mo1—O5—Na | −64.1 (13) |
O3i—Ni—O2—Mo1 | 79.6 (3) | O1—Mo1—O5—Na | −29.6 (8) |
O3—Ni—O2—Mo1 | −100.4 (3) | OW3—Na—O5—Mo1 | 146.3 (7) |
O8—Mo3—O2—Ni | 167.5 (4) | OW1—Na—O5—Mo1 | 58.2 (18) |
O9—Mo3—O2—Ni | −42.6 (11) | O12i—Na—O5—Mo1 | −17.1 (8) |
O10—Mo3—O2—Ni | 71.1 (3) | O11ii—Na—O5—Mo1 | −125.3 (7) |
O7—Mo3—O2—Ni | −91.5 (3) | O8—Mo3—O7—Mo1 | 72.6 (4) |
O3—Mo3—O2—Ni | 0.0 (3) | O9—Mo3—O7—Mo1 | 178.1 (4) |
O8—Mo3—O2—Mo1 | −88.5 (3) | O10—Mo3—O7—Mo1 | −55.5 (8) |
O9—Mo3—O2—Mo1 | 61.4 (11) | O2—Mo3—O7—Mo1 | −15.7 (3) |
O10—Mo3—O2—Mo1 | 175.0 (3) | O3—Mo3—O7—Mo1 | −89.5 (4) |
O7—Mo3—O2—Mo1 | 12.5 (3) | O6—Mo1—O7—Mo3 | −75.0 (4) |
O3—Mo3—O2—Mo1 | 104.0 (3) | O5—Mo1—O7—Mo3 | −179.9 (4) |
O6—Mo1—O2—Ni | −167.9 (3) | O4—Mo1—O7—Mo3 | 52.8 (8) |
O5—Mo1—O2—Ni | 37.4 (10) | O2—Mo1—O7—Mo3 | 15.7 (3) |
O4—Mo1—O2—Ni | −70.9 (3) | O1—Mo1—O7—Mo3 | 90.4 (4) |
O7—Mo1—O2—Ni | 92.5 (3) | O11—Mo2—O10—Mo3 | −73.9 (5) |
O1—Mo1—O2—Ni | 1.4 (3) | O12—Mo2—O10—Mo3 | −180.0 (4) |
O6—Mo1—O2—Mo3 | 87.2 (3) | O4i—Mo2—O10—Mo3 | 53.2 (8) |
O5—Mo1—O2—Mo3 | −67.5 (10) | O3—Mo2—O10—Mo3 | 16.4 (3) |
O4—Mo1—O2—Mo3 | −175.9 (3) | O1i—Mo2—O10—Mo3 | 90.3 (4) |
O7—Mo1—O2—Mo3 | −12.5 (3) | O8—Mo3—O10—Mo2 | 178.4 (4) |
O1—Mo1—O2—Mo3 | −103.5 (3) | O9—Mo3—O10—Mo2 | 72.9 (5) |
O1—Ni—O3—Mo2 | 179.1 (3) | O7—Mo3—O10—Mo2 | −52.6 (9) |
O1i—Ni—O3—Mo2 | −0.9 (3) | O2—Mo3—O10—Mo2 | −90.0 (4) |
O2i—Ni—O3—Mo2 | 80.1 (3) | O3—Mo3—O10—Mo2 | −16.4 (3) |
O2—Ni—O3—Mo2 | −99.9 (3) | O12—Mo2—O11—Naiii | −46 (2) |
O1—Ni—O3—Mo3 | −81.0 (3) | O4i—Mo2—O11—Naiii | 59 (2) |
O1i—Ni—O3—Mo3 | 99.0 (3) | O10—Mo2—O11—Naiii | −144 (2) |
O2i—Ni—O3—Mo3 | −180.0 (3) | O3—Mo2—O11—Naiii | 144 (2) |
O2—Ni—O3—Mo3 | 0.0 (3) | O1i—Mo2—O11—Naiii | 107 (2) |
O11—Mo2—O3—Ni | −168.8 (4) | O11—Mo2—O12—Nai | 140.2 (7) |
O12—Mo2—O3—Ni | 38.9 (10) | O4i—Mo2—O12—Nai | 38.6 (8) |
O4i—Mo2—O3—Ni | −71.2 (3) | O10—Mo2—O12—Nai | −117.8 (7) |
O10—Mo2—O3—Ni | 91.7 (4) | O3—Mo2—O12—Nai | −68.5 (13) |
O1i—Mo2—O3—Ni | 0.8 (3) | O1i—Mo2—O12—Nai | −32.3 (7) |
Symmetry codes: (i) −x+1, −y, −z; (ii) x+1, −y+1/2, z+1/2; (iii) x−1, −y+1/2, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N—HN1···O10 | 0.84 | 1.88 | 2.681 (12) | 157 |
N—HN2···O9iv | 0.93 | 2.03 | 2.830 (12) | 143 |
N—HN3···O5v | 0.84 | 2.06 | 2.883 (12) | 164 |
N—HN4···O12vi | 0.84 | 2.01 | 2.826 (12) | 164 |
O1—H1···O6vii | 0.87 | 1.98 | 2.847 (10) | 169 |
O2—H2···OW2 | 0.88 | 1.82 | 2.649 (11) | 156 |
O3—H3···O8vii | 0.87 | 1.91 | 2.781 (11) | 171 |
OW1—HW1B···O10viii | 0.85 | 2.34 | 3.074 (14) | 146 |
OW2—HW2B···O7v | 0.91 | 2.18 | 2.864 (10) | 131 |
OW3—HW3A···O9ix | 0.86 | 2.36 | 2.891 (13) | 121 |
OW3—HW3B···O4vii | 0.84 | 2.13 | 2.690 (12) | 124 |
Symmetry codes: (iv) x, −y+1/2, z+1/2; (v) −x+1, y−1/2, −z+1/2; (vi) −x, −y, −z; (vii) x, −y+1/2, z−1/2; (viii) x+1, y, z; (ix) −x+1, −y+1, −z. |
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